摘要
建立了同时测定鸡组织中残留的磺胺对甲氧嘧啶(SMD)和二甲氧苄啶(DVD)了的高效液相色谱-串联质谱法(HPLC-MS/MS)。样品经乙腈提取,取部分提取液用正己烷脱脂后于氮气吹干,残渣用流动相溶解并定容后上机检测,外标法定量。采用C18色谱柱,流动相为乙腈和1mL/L甲酸水溶液。选择1个母离子和2个子离子进行反应监测,对磺胺对甲氧嘧啶和二甲氧苄啶残留进行定性,选择信号最强的子离子进行定量。结果显示,SMD和DVD分别在1ng/mL^200ng/mL和0.5ng/mL^100ng/mL范围内呈良好线性关系,相关系数R2>0.992。通过空白样品添加回收试验,所有基质中SMD和DVD的定量限分别为10μg/kg和5μg/kg,SMD和DVD分别在50、100、200μg/kg和25、50、100μg/kg 3个添加水平下的回收率为71.7%~115.0%,相对标准偏差为1.8%~13.2%,该方法定量限低,灵敏度高,重现性好,符合相关研究的要求。
A high performance liquid chromatographic tandem mass spectrometry （LC-MS/MS） method was presented for simultaneous determination of sulfametoxydiazine and diaveridine residues in chicken. The samples were extracted with acetonitrile, then part of the extracts were cleaned up by n-hexane, fol- lowed by blowing to dryness under nitrogen gas stream,reconstitution with mobile phase before the analy- sis on HPLC-MS/MS using external standard method. The separation of analytes was performed on C18 analytical chromatographic column with a gradient elution using acetonitrile （A） and 1 mL/L formic acid （B） solution as mobile phase.The analysis of sulfametoxydiazine and diaveridine was performed under selective reaction monitoring（SRM） mode by selecting one parent ion and two daughter ions as qualitative i- ons, and the most abundant daughter ion as a quantitative ion. The calibration curves of SMD and DVD were linear in the concentration range of 1 ng/mL-200 ng/mL and 0.5 ng/mL-100 ng/mL respectively, with correlation coefficients more than 0.992.The quantitative limits of the method for SMD and DVD were 10μg/kg and 5 μg/kg respectively for all matrices,and the recoveries were in the range of 71.7%-115.0% with RSDs of 1.8%-13.2% while blank samples were spiked with sulfametoxydiazine and diaveridine at 50, 100,200μg/kg and 25,50,100 μg/kg, respectively. This analytical method meets the requirements for as- says.
出处
《动物医学进展》
北大核心
2016年第7期57-63,共7页
Progress In Veterinary Medicine
基金
农业部兽药行业标准制定和修订项目[农财发(2013)46号-32]
